Reacción #3043

ord-5ea8ac69bd1848ae813a64e74a7a7adf

Condiciones de reacción

Temperatura
-4°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    OtroThe mixture separated into layers which
  2. 2
    Otrowere subsequently separated
  3. 3
    LavadoThe organic layer was washed with 100 ml of saturated sodium bicarbonate and 100 ml of brine
  4. 4
    OtroThe organic layer was dried
  5. 5
    Otrothe solvent evaporated

Procedimiento

Under a nitrogen atmosphere, 6.89 ml of acetylchloride and 14.75 ml of stannic chloride were dissolved in 200 ml of methylene chloride and chilled to -4° C. To this was added 20 g of 2,6-di-t-butylphenol (in 100 ml of methylene chloride) over 10 minutes. The resultant mixture was stirred for 30 minutes at 0° C., then poured into a mixture of 400 ml of ice and 1N hydrochloric acid and stirred. The mixture separated into layers which were subsequently separated. The organic layer was washed with 100 ml of saturated sodium bicarbonate and 100 ml of brine. The organic layer was dried and the solvent evaporated to give 23.39 g of the desired subtitled intermediate.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US05731336uspto-grants-1998_03